六神丸和日本救心丹中挥发性成分的GC/MS分析

Analysis of the volatile compounds in Liushen Pill and Japannese Jiuxin Pill by GC/MS

目的:采用GC/MS技术,以六神丸和日本救心丹为例,对其挥发性成分进行研究。方法:色谱柱为CP8944 VF-5ms,30 m×0.25 mm;气相部分采用分流进样,进样口温度280℃,载气流速1 mL/min,传输线温度250℃;质谱部分采用EI/MS模式,以外标法为定量方法。溶剂延迟6 min,平均扫描速度为0.87 sencond/scan,灯丝电流80 mA,离子阱和歧管分别为170℃,45℃。结果:定量方法的基质干扰少,线性范围宽,其中麝香酮的检出限可达到4 ppb,并采用单一标准品代替相似结构物质的定量方式定量了异龙脑的含量。结论:GC/MS为中药复杂体系中挥发性成分的定性定量分析提供了一种准确、灵敏、有效的手段。

AIM： To develop a GC/MS method for analyzing volatile compounds in Liushen Pill and Japanese Jiuxin Pill. METHODS： The gas chromatograph was fitted a fused-silica capillary column with a VF-5 ms stationary phase and dimensions：30 m ×0.25 mm i. d. ,0.25 μm film thickness. The carrier gas was helium at a flow-rate of 1 mL/min. Injector temperature was at 280 ℃ and operated in the splitless mode. The temperature of the GC-MS transfer line was at 250 ℃. Full scan electron impact ionization data were acquired under the following condition ： solvent delay 6 min. 70 eV electron impact energy, scan time 0.87 sencond/scan, emission current 80 mA, manifold and trap temperatures 45 ℃ and 170 ℃. RESULTS： The quantitative method was accepted with good specificity, wide linear range and low LOD. At the same time, the content of isoborneol was determined by a semi-quantitative approach. CONCLUSION： The research is propitious to offer an effective and reliable pattern for analyzing volatile compounds in complex composite formulae.